Reaktion #2507821

Reaktionsgleichung

potassium hydride

3-(4-bromo-2,5-difluorophenyl)-2-(6-fluoro-3-propylchroman-7-yl)propan-1-ol

ethanol

→

7-bromo-6,6′-difluoro-3′-propyl-3,4,3′,4′-tetrahydro-2H,2′H-[3,7′]-bichromenyl

Lösungsmittel

ether

THF

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with sat. sodium chloride soln
2. 2
   Trocknenphase is dried over sodium sulfate
3. 3
   Sonstigethe solvent is removed in vacuo
4. 4
   Filtrationthe crude product is filtered through silica gel with toluene
5. 5
   Sonstigerecrystallised from heptane/ethyl acetate

Vorschrift

1.2 g (10.5 mmol) of potassium hydride (35 percent in paraffin oil) are initially introduced in 40 ml of THF, and a solution of 4.50 g (8.12 mmol) of 3-(4-bromo-2,5-difluorophenyl)-2-(6-fluoro-3-propylchroman-7-yl)propan-1-ol in 20 ml of THF is added dropwise at 30° C. The batch is subsequently stirred at 60° C. for 4 h, a little ethanol is added, and the batch is diluted with MTB ether and washed with sat. sodium chloride soln. The org. phase is dried over sodium sulfate, the solvent is removed in vacuo, and the crude product is filtered through silica gel with toluene and recrystallised from heptane/ethyl acetate, giving 7-bromo-6,6′-difluoro-3′-propyl-3,4,3′,4′-tetrahydro-2H,2′H-[3,7′]-bichromenyl as colourless crystals.

Quelle